反应详情

温度

55 °C

To a mixture of 3-hydroxy-thiophene-2-carboxylic acid methyl ester (5 g, 31.6 mmol) and K2CO3 (22.2 g, 161 mmol) in acetone (50 mL) is added CH3I (10.8 mL, 173 mmol,) dropwise at 0° C. The reaction mixture is heated at 55° C. for 4 hours, cooled to room temperature, filtered through diatomaceous earth, and the filtrate is concentrated under vacuum. The residue is diluted with water (100 mL) and extracted with ethyl acetate (2×200 mL). The combined organic layer is washed with brine solution (50 mL), dried over Na2SO4, and evaporated under vacuum to give title compound as a brown solid (5.9 g). ESI/MS m/z 173.1 (M+H)+.

1. temperaturecooled to room temperature
2. filtrationfiltered through diatomaceous earth
3. concentrationthe filtrate is concentrated under vacuum
4. additionThe residue is diluted with water (100 mL)
5. extractionextracted with ethyl acetate (2×200 mL)
6. washThe combined organic layer is washed with brine solution (50 mL)
7. dry with materialdried over Na2SO4
8. customevaporated under vacuum